Dyestuff preparation and process of making same



Patented Aug. 11, 1931- UNITED STATES ADAM ARBOGAST,

or BASEL, SWITZERLAND, Assmnon 'ro INDUSTRY IN BAs'LE, or BASEL, SWITZERLAND SOCIETY OF CHEMICAL nxus'rurr PREPARATION, AND raocuss ormxme sum no Drawing. Application filed June 15, 1928, Serial No. 285,792, and in Switzerland June 24, 1927.

The present invention relates to new dyest-utf preparations, particularly suitable for p producing fast tints on the fibre. It comprises the new preparations, the process of making same, and the materialthat has been dyed with the new products.

The symmetrical 1:2- and 2: l-napththioindigoes are described in literature as brown Nothing 'more concerning which are not commercial When these dyestufis are 1 2-napthth io-indi- -napththio-indivat-dyestuffs. these compounds, products, is known. made it is found that the go is a red-brown and; the 2: go is more yellow brown. r

r This invention is based onthe observation that when these dyestufi's are mixed either by mechanically mixing them or by oxidizing the mixed corresponding leucocompounds or ester salts of the leuco-compounds, or a mixture of the corresponding hydroxy-thionaphthene derivatives-which may be carried out either in substance or on the.fibre-new products are obtained which dye fibres brown tints, the fullness and brightness of which essentially exceeds those which could be expected from the dyeings of the components The effect is already perceptible when one of the dyein a suitable apparatus.

' er and fuller.

stuffs contains only a few percents of the other.

The same result is obtained when the vats of the separate dyestuffs are mixed or mixtures of the leuco-compounds or of the ester salts of the leuco-compounds of the respective dyestuffs are used. Obviously the new products themselves can be converted into leucocompounds or ester salts thereof and, then brought into use.

The following examples illustrate the invention, the parts being by weight Example 1 30 parts of 1 2-napththio-indigo are mixed with 70 parts of 2i1-napththio-indigo The product dyes cotton in a vat red-brown similar, to the tints produced-by pure 1:2- napththioeindigobut are considerably bright- Instead of a mixture made mechanically'there may be used one which is prepared in a chemical manner, for instance tints which are.

at 70-80 G. are add by oxidizing the mixtures ounds or the corresponding hydroxy-thionaphthene derivatives.

Similar products are obtained if the proportion in which the components are mixed is varied in one direction or the other. The dyeings can be discharged by hydrosulfite.

Example 2 To a mixture of 1100 parts of chlorobenzene and 535 arts of dimethylaniline are added at 0-2 245 parts of chlorosulfonic acid. Into this mixture there are, introduced, while maintaining an atmosphere of carbon dioxide and stirring at a temperature of 0 C., 398 parts of the dry leuco-compound of a mixture of equal welghts of 1:- and of the leuco-com- 2:1-napththio-indigo corresponding proba-.

and

solution and distilled in steam. The contents of the still are then concentrated in a vacuum,- common salt is added to the li uid and the sodium salt of the new product t us obtained is filtered and dried.

Example 3 A mixture of 600 grams of 2: 1 napththioindigo and 400 grams of lz2-napththio-indigo is made into a paste with 1 kilo of a highly sulfonated castor oil and litres of water ed; 3 litres of caustic soda solution of 36 B6. are then added and 1 hour at 90 C.

2.5 kilos of hydrosulfite conc. powder are scattered into the liquid. Vatting is'completed after 10 minutes.

Instead of using the dyestufi' in the form of a powder it may be vatted in the form of a paste. For the highly sulfonated castor oil ma be substituted another wetting agent, such as a less highly sulfonated castor oil or sulfite cellulose waste liquor freed from lime. The dyeing vat is now made up with 1000 litres of water and 1000-250 0. c. of caustic soda solution of 36 B., and the whole is heated to 60 0., separated lime is removed if necessary and hydrosulfite conc. powder added according to the depth of tint required. In general, there is used for light tints 1 kilo, for medium tints 0.5 kilo and for dark tints 0.2 kilo -of hydrosulfite conc. powder per 1000 litres of vat. The stockvat and the dye-vat are now united, the well boiled and wetted cotton is introduced and dyeing conducted for hour at 60 C. For exhausting the dye-bath there are added after 4 hour dyeing 10 to grams of common salt dissolved in water er litre of vat. After the dyeing the goo s are wrung out, suspended for oxidation, washed, soured and developed by boiling with 3 grams of soap and 1 gram' of calcined sodium carbonate per litre of water for ,4,; hour.

A like prescription serves for applying the product in piece-dyeing.

Example 4 The stock-vat is prepared as described in Example 3, except that in this case half the quantity of a highly sulfonated castor oil 2 litres of caustic soda solution of 36 B. and-11.5 kilo ofhydrosulfite conc. powder are use a To the dye-bath, heated to 5060 (3., are added 500 grams of glue (swollen and freshly dissolved) or another protective colloid, 500 cc. of ammonia of 20 er cent. strength and 300 grams of hydrosulhte conc. powder per 1000 litres of water. (For light tints up to 1 per cent. there are also added 500 cc. of caustic soda solution of 36 B6. and 200 grams of hydrosulfite conc. powder.) The dissolved dyestuif is then added through a fine sieve and the whole is stirred; the dry or wetted wool is entered and dyeing is continued for y 'hour at 5060 C. The goods are then wrung out, oxidized in the air washed and develo ed with 1 to 2 cc. of sulfuric acid of 66, per litre of water for If silk is to be dyed instead of wool the operation is conducted accordin to Exisifliple 3 but without the addition 0 common Emample 5 For printing theusual method for Ciba a... is adopted with a printing colour which is feebly alkaline or contains only potash: for example- 100 grams of the product described in the first paragraph of Exarlxliple 1 in the form of a paste of 20 per cent.

strengt 600 grams of potash thickening 30 grams of caustic soda solution of 36" Be.

20 grams-of hydrosulfite conc. powder are heated together at 50 to 60 C. until reduction has occurred and there are added 50 gran}?i of dthe sodium salt of formaldehydesulfoxylic c an a 200 grams of water,

1 kilo,

100 grams of the product of the first para-graph of Example 1 in the form of a pasteof 20 per cent. strength 600 grams of potash thickening 200 grams of water,

60 grams of the sodium salt of formaidehydesultoxylic The goods are printed withthe following printing colour 40 grams of the product of Example 2 340 grams of water vI500 grams of tragacanth thickening 5-20 grams of sodium nitrite 100 grams of water 1 kilo The goods are then dried, developed in a warm sulfuric acid bathv which contains about cc. of sulfuric acid of 66 B. per litre, washed, neutralized and soaped.

Example 7 The goods ore printed with printing colour grams of a mixture of equal parts sailts of 1:

the following of the leuco-ester 2- and 2:1-napththio-indigo 330 grams of water 450 grams of neutral starch tra-gacantli thickening grams of sodium chlorate solution 1:3 30 grams of ammonium sulfocyanide solution 1:1 100 grams of ammonium vanadate 1 1000 1 kilo.

They are then dried, treated in the Mather- Platt apparatus, washed and soaped.

Theleuco-ester salts also dye animal fibre in an acid bath and may subsequently be firolilight to full development in an oxidizing What we claim is 1. As new products dyestufi preparations,

napththio-indigoes to obtain a coloring matter yielding on the fibres brown tints of greater fullness and brightness than those consisting in' amixture of 2:1- and '112- which could be expected from the mixture oft-he components.

2. In the preparation of dyestufi prepare tions, the process consisting in mixing symmetrical 1 2-napththio-ind1 0 with'symmetrica1.2:1-napththio-indi o %y oxidizing together a mixture of the euco-compoun s of said dyestuffs.

3. In the preparation of dyestuff preparations, the process consisting in mixing symmetrical 1:2-napththio-ind1 o with symmetrical 2:1-napththio-indi o y oxidizing together a mixture of the euco-compounds of said dyestuffs on textile material.

In witness whereof I have hereunto signed my name this 5th day of June, 1928.

. ADAM ARBOGAST. 

